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1.
Natural Deep Eutectic Solvent-Based Matrix Solid Phase dispersion (MSPD) extraction for determination of bioactive compounds from sandy everlasting (Helichrysum arenarium L.) : a case of stability study
Milena Ivanović, Peter Krajnc, Aleš Mlinarič, Maša Islamčević Razboršek, 2022, izvirni znanstveni članek

Opis: In the present study, vortex-assisted matrix solid-phase dispersion (VA-MSPD) extraction was used to isolate the major bioactive compounds from H. arenarium. To reduce the negative environmental impact of the conventionally used organic solvents, four different choline chloride-based natural deep eutectic solvents (NADES) were investigated as possible eluents. The most influential VA-MSPD extraction parameters: stationary phase (adsorbent), adsorbent/sample ratio, vortex time, and volume of extraction solvent were systematically optimized. Ultrasound-assisted extraction with 80% MeOH was used as the standard method for the comparison of results. The stability of the obtained extracts was studied over a period of 0 to 60 days at three different temperatures (−18 ◦C, 4 ◦C, and 25 ◦C). All extracts were evaluated both spectrophotometrically (determination of total phenolic content (TPC) and antioxidant activity by ABTS and FRAP assay) and chromatographically (HPLC-UV). NADES based on choline chloride and lactic acid (ChCl-LA) was selected as the most effective extractant, with a determined TPC value of its extract of 38.34 ± 0.09 mg GA/g DW (27% higher than the methanolic VA-MSPD extract) and high antioxidant activity. The content of individual phenolic compounds (chlorogenic acid, dicaffeoylquinic acid isomers, naringenin isomers, and chalcones) in the ChCl-LA extract, determined by HPLC-UV, was comparable to that of the conventionally obtained one. Moreover, the stabilization effect of ChCl-LA was confirmed for the studied compounds: chlorogenic acid, naringenin-40 -O-glucoside, tomoroside A, naringenin-5-Oglucoside, isosalipurposide, and naringenin. The optimum VA-MSPD conditions for the extraction of H. arenarium polyphenols were: florisil/sample ratio of 0.5/1, a vortex time of 2 min, and an elution volume of ChCl-LA of 10 mL.
Ključne besede: matrix solid phase dispersion extraction, MSPD, natural deep eutectic solvents, NADES, extraction optimization, sandy everlasting, phenolic compounds, stability studies, antioxidant activity
Objavljeno v DKUM: 09.05.2025; Ogledov: 0; Prenosov: 3
.pdf Celotno besedilo (2,47 MB)
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2.
Extraction of bioactive metabolites from Achillea millefolium L. with choline chloride based natural deep eutectic solvents: a study of the antioxidant and antimicrobial activity
Milena Ivanović, Dragana Grujić, Janez Cerar, Maša Islamčević Razboršek, Ljiljana Topalić-Trivunović, Aleksandar Savić, Drago Kočar, Mitja Kolar, 2022, izvirni znanstveni članek

Opis: In this study, the extraction efficiency of natural deep eutectic solvents (NADES) based on choline chloride as a hydrogen bond acceptor (HBA) and five different hydrogen bond donors (HBD; lactic acid, 1,4-butanediol, 1,2-propanediol, fructose and urea) was evaluated for the first time for the isolation of valuable bioactive compounds from Achillea millefolium L. The phytochemical profiles of NADES extracts obtained after ultrasound-assisted extraction were evaluated both spectrophotometrically (total phenolic content (TPC) and antioxidant assays) and chromatographically (UHPLC-MS and HPLC-UV). The results were compared with those obtained with 80% ethanol, 80% methanol, and water. The highest TPC value was found in the lactic acid-based NADES (ChCl-LA), which correlated with the highest antioxidant activity determined by the FRAP analysis. On the other hand, the highest antiradical potential against ABTS$^{+•}$ was determined for urea-based NADES. Phenolic acids (chlorogenic acid and dicaffeoylquinic acid isomers), flavones (luteolin and apigenin), and their corresponding glucosides were determined as the dominant individual phenolic compounds in all extracts. The antibacterial and antifungal properties of the extracts obtained against four bacterial cultures and two yeasts were evaluated using two methods: the agar dilution method to obtain the minimum inhibitory concentration (MIC) and the minimum bactericidal or fungicidal concentration (MBC or MFC), and the disc diffusion method. ChCl-LA had the lowest MIC and MBC/MFC with respect to all microorganisms, with an MIC ranging from 0.05 mg mL$^{−1}$ to 0.8 mg mL$^{−1}$, while the water extract had the weakest inhibitory activity with MIC and MBC/MFC higher than 3.2 mg mL$^{−1}$.
Ključne besede: viskoznost, fenoli, antioksidanti, natural deep eutectic solvents (NADES), density and viscosity, yarrow, phenolic compounds, antioxidant activity, antimicrobial activity
Objavljeno v DKUM: 09.04.2025; Ogledov: 0; Prenosov: 3
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3.
Effect of micro- and nano-lignin on the thermal, mechanical, and antioxidant properties of biobased PLA–lignin composite films
Sofia P. Makri, Eleftheria Xanthopoulou, Panagiotis A. Klonos, Alexios Grigoropoulos, Apostolos Kyritsis, Konstantinos Tsachouridis, Antonios Anastasiou, Ioanna Deligkiozi, Nikolaos P. Nikolaidis, Dimitrios Bikiaris, 2022, izvirni znanstveni članek

Opis: Bio-based poly(lactic acid) (PLA) composite films were produced using unmodified soda micro- or nano-lignin as a green filler at four different contents, between 0.5 wt% and 5 wt%. The PLA– lignin composite polymers were synthesized by solvent casting to prepare a masterbatch, followed by melt mixing. The composites were then converted into films, to evaluate the effect of lignin content and size on their physicochemical and mechanical properties. Differential scanning calorimetry (DSC), supported by polarized light microscopy (PLM), infrared spectroscopy (FTIR-ATR), X-ray diffraction (XRD), and transmission electron microscopy (TEM) were employed to investigate the PLA crystallization and the interactions with Lignin (L) and Nanolignin (NL). The presence of both fillers (L and NL) had a negligible effect on the glass transition temperature (chain diffusion). However, it resulted in suppression of the corresponding change in heat capacity. This was indicative of a partial immobilization of the PLA chains on the lignin entities, due to interfacial interactions, which was slightly stronger in the case of NL. Lignin was also found to facilitate crystallization, in terms of nucleation; whereas, this was not clear in the crystalline fraction. The addition of L and NL led to systematically larger crystallites compared with neat PLA, which, combined with the higher melting temperature, provided indications of a denser crystal structure in the composites. The mechanical, optical, antioxidant, and surface properties of the composite films were also investigated. The tensile strength and Young’s modulus were improved by the addition of L and especially NL. The UV-blocking and antioxidant properties of the composite films were also enhanced, especially at higher filler contents. Importantly, the PLA–NL composite films constantly outperformed their PLA–L counterparts, due to the finer dispersion of NL in the PLA matrix, as verified by the TEM micrographs. These results suggest that bio-based and biodegradable PLA films filled with L, and particularly NL, can be employed as competitive and green alternatives in the food packaging industry.
Ključne besede: poly(lactic acid), PLA, lignin, nanolignin, composite films, nucleation, mechanical properties, antioxidant activity, food packaging
Objavljeno v DKUM: 26.03.2025; Ogledov: 0; Prenosov: 1
.pdf Celotno besedilo (9,96 MB)
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4.
Comparison of conventional and supercritical isolation methods from bee pollen and their effects on the concentrations of bioactive compounds
Taja Žitek Makoter, Vesna Postružnik, Anastasia Kyriakoudi, Elli Pantazi, Natasa Kalogiouri, Ioannis Mourtzinos, Željko Knez, Maša Knez Marevci, 2025, izvirni znanstveni članek

Opis: The present work represents a profound investigation of material pretreatment, comparison of different isolation methods (conventional and supercritical), and characterization of phenolic compounds and amino acids from bee pollen. The determination of amino acids was carried out after developing a novel hydrophilic interaction chromatography combined with quadrupole time-of-flight tandem mass spectrometric method (HILIC-QTOF-MS/MS) with limits of detection over the range 1 mg/kg -5 mg/kg and recoveries over the range 87.6% - 97.1%. The optimal conditions for the isolation of amino acids are in the range of temperatures between 25°C to 55°C and at pressures between 300 bar and 350 bar. It can be concluded that the extraction temperature and the pressure affect antioxidant activity. The favored conditions are lower temperatures and higher pressures.
Ključne besede: bee pollen, in vitro antioxidant activity, HILIC-LC-QTOF-MS.MS, amino acids, WM-266-4 cells
Objavljeno v DKUM: 20.03.2025; Ogledov: 0; Prenosov: 2
.pdf Celotno besedilo (1,27 MB)

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Eco-finishing of cotton with chitosan and giant goldenrod (Solidago gigantea Aiton) aqueous extract for development of antioxidant and UV protective textiles
Sebastijan Šmid, Anja Verbič, Lidija Fras Zemljič, Marija Gorjanc, 2023, izvirni znanstveni članek

Opis: Giant goldenrod (S. gigantea Aiton) is considered an invasive weed in Europe, Asia, Australia, and New Zealand. In this research, the untreated and chitosan-treated cotton fabrics were functionalized with goldenrod inflorescences aqueous extract, at room temperature and 95°C. Zeta potential of fabrics was determined as a function of pH and the results showed an increased isoelectric point from 2.50 to 5.25 and amphoteric character of the chitosan-treated sample. The antioxidant activity (AA) of extract and functionalized fabrics was determined using DPPH analysis, while color and ultraviolet protection factor (UPF) were determined spectroscopically before and after wash and lightfastness testing. The chitosan pretreatment and dyeing of cotton at higher temperature increased AA (from 41.19 ± 0.28 to 56.08 ± 0.25), UPF (from 33.05 to 51.59) and color strength (K/S) (from 1.74 to 2.21), providing dyed cotton with excellent UV protection and a free radical inhibition activity. The samples had good wash fastness in terms of color (ΔEab* < 1), but not in terms of UV protection (UPF value decreased after washing to 23.47). The overall lightfastness was good to excellent (the UPF values of chitosan and dyed samples did not change much after lightfastness test (UPF = 51.75).
Ključne besede: Goldenrod, invasive plant, eco-functionalisation, cotton, antioxidant activity, UV protection
Objavljeno v DKUM: 25.03.2024; Ogledov: 255; Prenosov: 27
.pdf Celotno besedilo (1,89 MB)
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8.
Antioxidant activity of different hop (Humulus lupulus L.) genotypes
Zala Kolenc, Tamara Hribernik, Tomaž Langerholc, Maša Pintarič, Maja Prevolnik Povše, Urban Bren, 2023, izvirni znanstveni članek

Opis: The antioxidant activity (AA) of hop extracts obtained from different hop genotypes (n = 14) was studied. For comparison, the purified β-acids-rich fraction and α-acids-with-β-acids-rich fraction were also used to test the antioxidative potential. The AA of purified hydroacetonic hop extracts was investigated using the Ferric Reducing Ability of Plasma (FRAP), Oxygen Radical Absorption Capacity (ORAC) and Intracellular Antioxidant (IA) methods. The FRAP values in different hop genotypes ranged between 63.5 and 101.6 μmol Trolox equivalent (TE)/g dry weight (DW), the ORAC values ranged between 1069 and 1910 μmol TE/g DW and IA potential values ranged between 52.7 and 118.0 mmol TE/g DW. Significant differences in AA between hop genotypes were observed with all three methods. AAs were determined using three different methods, which did not highly correlate with each other. We also did not find significant correlations between AA and different chemical components, which applies both to AA determined using individual methods as well as the total AA. Based on this fact, we assume that the synergistic or antagonistic effects between hop compounds have a more pronounced effect on AA than the presence and quantity of individual hop compounds.
Ključne besede: hop, antioxidant activity, FRAP, ORAC, intracellular antioxidative potential, genotypes
Objavljeno v DKUM: 20.03.2024; Ogledov: 271; Prenosov: 19
.pdf Celotno besedilo (1,23 MB)
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9.
Kraft lignin/tannin as a potential accelerator of antioxidant and antibacterial properties in an active thermoplastic polyester-based multifunctional material
Klementina Pušnik Črešnar, Alexandra Zamboulis, Dimitrios Bikiaris, Alexandra Aulova, Lidija Fras Zemljič, 2022, izvirni znanstveni članek

Opis: This research focuses on key priorities in the field of sustainable plastic composites that will lead to a reduction in CO2 pollution and support the EU’s goal of becoming carbon neutral by 2050. The main challenge is to develop high-performance polyphenol-reinforced thermoplastic composites, where the use of natural fillers replaces the usual chemical additives with non-toxic ones, not only to improve the final performance but also to increase the desired multifunctionalities (structural, antioxidant, and antibacterial). Therefore, poly (lactic acid) (PLA) composites based on Kraft lignin (KL) and tannin (TANN) were investigated. Two series of PLA composites, PLA-KL and PLA-TANN, which contained natural fillers (0.5%, 1.0%, and 2.5% (w/w)) were prepared by hot melt extrusion. The effects of KL and TANN on the PLA matrices were investigated, especially the surface physicochemical properties, mechanical properties, and antioxidant/antimicrobial activity. The surface physicochemical properties were evaluated by measuring the contact angle (CA), roughness, zeta potential, and nanoindentation. The results of the water contact angle showed that neither KL nor TANN caused a significant change in the wettability, but only a slight increase in the hydrophilicity of the PLA composites. The filler loading, the size of the particles with their available functional groups on the surfaces of the PLA composites, and the interaction between the filler and the PLA polymer depend on the roughness and zeta potential behavior of the PLA-KL and PLA-TANN composites and ultimately improve the surface mechanical properties. The antioxidant properties of the PLA-KL and PLA-TANN composites were determined using the DPPH (2,2′-diphenyl-1-picrylhydrazyl) test. The results show an efficient antioxidant behavior of all PLA-KL and PLA-TANN composites, which increases with the filler content. Finally, the KL- and PLA-based TANN have shown resistance to the Gram-negative bacteria, E. coli, but without a correlation trend between polyphenol filler content and structure.
Ključne besede: poly (lactic acid), Kraft lignin, tannin, multifunctionality of PLA composites, surface mechanical properties, antioxidant/antibacterial activity
Objavljeno v DKUM: 18.09.2023; Ogledov: 495; Prenosov: 193
.pdf Celotno besedilo (3,87 MB)
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10.
Green techniques for preparation of red beetroot extracts with enhanced biological potential
Dragana Borjan, Vanja Šeregelj, Darija Cör Andrejč, Lato Pezo, Vesna Tumbas Šaponjac, Željko Knez, Jelena J. Vulić, Maša Knez Marevci, 2022, izvirni znanstveni članek

Opis: Red beetroot is well known for its high proportion of betalains, with great potential as functional food ingredients due to their health-promoting properties. The objective of this study was to investigate the influence of processing techniques such as Soxhlet, cold, ultrasound and supercritical fluid extraction on the betalains content and its antioxidant, anti-inflammatory and antihyperglycemic activities. Whilst Soxhlet extraction with water has provided the highest yield, the highest content of total phenolics was found in an extract prepared using Soxhlet extraction with 50% ethanol. Amongst eight phenolic compounds detected in the extracts, protocatechuic acid was the most abundant. The concentrations of total phenolics ranged from 12.09 mg/g (ultrasound extraction with 30% methanol) to 18.60 mg/g (Soxhlet extraction with 50% ethanol). The highest anti-inflammatory activity was observed for cold extraction with 50% methanol extract. The high radical scavenging activity of supercritical fluid extracts could be a consequence of nonphenolic compounds. The chemometrics approach was further used to analyse the results to find the “greenest” method for further possible application in the processing of beetroot in the food and/or pharmaceutical industry. According to the standard score, the best extraction method was determined to be Soxhlet extraction with 50% ethanol.
Ključne besede: red beetroot, supercritical fluid extraction, antioxidant activity, anti-inflammatory activity, antihyperglycemic activity, chemometric approach
Objavljeno v DKUM: 18.08.2023; Ogledov: 436; Prenosov: 124
.pdf Celotno besedilo (944,05 KB)
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